Protection Against the Oxidation of Composite Material Parts Containing Carbon and Parts thus Protected
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example 1
[0054] Samples of C / C composite material were made as follows.
[0055] Unidirectional fiber sheets of carbon precursor fibers (preoxidized polyacrylonitrile) were superposed in different directions and bonded together by needling as the superposition was being built up. The resulting fiber preform was subjected to heat treatment to transform the precursor into carbon by pyrolysis, and was then densified with a pyrolytic carbon matrix by chemical vapor infiltration. Such a method is well known. Reference can be made, for example, to document U.S. Pat. No. 4,790,052. Samples in the form of rectangular blocks having dimensions of 20 mm×25 mm×8 mm were cut out from the block of C / C material obtained in this way.
[0056] Several samples were provided with protection against oxidation by a process comprising the following steps:
[0057] a) preliminary treatment of the samples by immersing them in an ultrasound vessel containing an aqueous solution of a wetting agent based on polyethoxyl ison...
example 2
[0081] The procedure was as in Example 1, but in step c), an impregnation composition was used containing, in percentage by weight, 32% of Al (H2PO4)3 and 56% ZrB2, the remainder being water.
[0082] Several samples protected using the method of Example 2 were subjected to an oxidation test identical to test V) above.
[0083] Table II below shows the relative mass losses measured on the various samples after performing the observation test (as a percentage relative to initial mass). By way of comparison, Table II shows the mass losses observed in the same oxidation test on samples protected in accordance with Example 1 and on reference protected samples.
TABLE II(Test 1 × 5 h − 650° C. + 1 × 20 min − 1200° +2 × 5 h − 650°)SamplesMass lossProtected in accordance with2.6%Example 12.6%3.4%Protected in accordance with10.1% Example 211.4% 12.5% Reference9.2% 13% 13%
[0084] The results show that using ZrB2 as a substitute for TiB2 in the impregnation composition leads to a significant loss ...
example 3
[0085] The samples used were made of C / C composite material of the same kind as in Example 1, and they were protected against oxidation by modifying the process described in Example 1 as follows:
[0086] in step b), an impregnation composition was used containing, in percentages by weight: 44% of Al (H2PO4)3 and 14% of TiB2 in powder form having a mean grain size of about 10 μm, the remainder being water; and
[0087] in step c), an impregnation composition was used containing, in percentages by weight: 34% of Al (H2PO4)3 and 39% of TiB2 in powder form having a mean grain size equal to about 10 μm.
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